Solid-State 65Cu and 31P NMR Spectroscopy of Bis(triphenylphosphine) Copper Species

Autor: Bryan E. G. Lucier, John V. Hanna, Robert W. Schurko, Joel A. Tang, Graham A. Bowmaker, Peter Conrad Healy
Rok vydání: 2010
Předmět:
Zdroj: The Journal of Physical Chemistry C. 114:7949-7962
ISSN: 1932-7455
1932-7447
Popis: Frequency-stepped ultrawideline (UW) 65Cu solid-state NMR (SSNMR) experiments have been performed on a series of nine bis(triphenylphosphine) copper(I) species, with eight of these having an oxyanion-based ligand and one a borohydride ligand. These copper atoms reside in spherically asymmetric environments featuring two covalent Cu−P bonds and coordination from single bidentate ligands. The QCPMG pulse sequence was utilized in NMR experiments on all of the samples, along with the WURST-QCPMG sequence on select samples, to acquire UWNMR spectra of high quality. In all cases, large 65Cu quadrupolar coupling constants (CQ) between 40.8 and 51.7 MHz are observed, and are confirmed by NQR measurements. The immense quadrupolar interactions and their correspondingly large contributions to the central-transition powder patterns make accurate quantification of copper chemical shift anisotropy (CSA) difficult, though CSA effects are observed. 1H−31P CP/MAS NMR spectra reveal one-bond J-couplings, 1J(65/63Cu, 31P), ...
Databáze: OpenAIRE